Monitoring of Curing and Cyclic Thermoresistive Response Using Monofilament Carbon Nanotube Yarn Silicone Composites
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Tannaz Tayyarian↗
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Resin Film Infusion (RFI) Process Modeling for Large Transport Aircraft Wing Structures
This investigation completed the verification of a three-dimensional resin transfer molding/resin film infusion (RTM/RFI) process simulation model. The model incorporates resin flow through an anisotropic carbon fiber preform, cure kinetics of the resin, and heat transfer within the preform/tool assembly. The computer model can predict the flow front location, resin pressure distribution, and thermal profiles in the modeled part. The formulation for the flow model is given using the finite element/control volume (FE/CV) technique based on Darcy's Law of creeping flow through a porous media. The FE/CV technique is a numerically efficient method for finding the flow front location and the fluid pressure. The heat transfer model is based on the three-dimensional, transient heat conduction equation, including heat generation. Boundary conditions include specified temperature and convection. The code was designed with a modular approach so the flow and/or the thermal module may be turned on or off as desired. Both models are solved sequentially in a quasi-steady state fashion. A mesh refinement study was completed on a one-element thick model to determine the recommended size of elements that would result in a converged model for a typical RFI analysis. Guidelines are established for checking the convergence of a model, and the recommended element sizes are listed. Several experiments were conducted and computer simulations of the experiments were run to verify the simulation model. Isothermal, non-reacting flow in a T-stiffened section was simulated to verify the flow module. Predicted infiltration times were within 12-20% of measured times. The predicted pressures were approximately 50% of the measured pressures. A study was performed to attempt to explain the difference in pressures. Non-isothermal experiments with a reactive resin were modeled to verify the thermal module and the resin model. Two panels were manufactured using the RFI process. One was a stepped panel and the other was a panel with two 'T' stiffeners. The difference between the predicted infiltration times and the experimental times was 4% to 23%.
Loos, Alfred C.↗
BLIMPK/Streamline Surface Catalytic Heating Predictions on the Space Shuttle Orbiter
This paper describes the results of an analysis of localized catalytic heating effects to the U.S. Space Shuttle Orbiter Thermal Protection System (TPS). The analysis applies to the High-temperature Reusable Surface Insulation (HRSI) on the lower fuselage and wing acreage, as well as the critical Reinforced Carbon-Carbon on the nose cap, chin panel and the wing leading edge. The object of the analysis was to use a modified two-layer approach to predict the catalytic heating effects on the Orbiter windward HRSI tile acreage, nose cap, and wing leading edge assuming localized highly catalytic or fully catalytic surfaces. The method incorporated the Boundary Layer Integral Matrix Procedure Kinetic (BLIMPK) code with streamline inputs from viscous Navier-Stokes solutions to produce heating rates for localized fully catalytic and highly catalytic surfaces as well as for nominal partially catalytic surfaces (either Reinforced Carbon-Carbon or Reaction Cured Glass) with temperature-dependent recombination coefficients. The highly catalytic heating results showed very good correlation with Orbiter Experiments STS-2, -3, and -5 centerline and STS-5 wing flight data for the HRSI tiles. Recommended catalytic heating factors were generated for use in future Shuttle missions in the event of quick-time analysis of damaged or repaired TPS areas during atmospheric reentry. The catalytic factors are presented along the streamlines as well as a function of stagnation enthalpy so they can be used for arbitrary trajectories.
Marichalar, Jeremiah J.↗
Pull-off Behavior of Stitched Composite T-Joints
T-joints are key structural elements that connect opposing surfaces, thereby providing the load path between flat or curved panels (i.e., upper and lower wing skins) and transverse components (i.e., stiffeners). Due to the low interlaminar strength of polymer matrix composites and their geometrical discontinuities, these joints are vulnerable to pull-off loads. To address these issues, through-thickness reinforcements can be employed to enhance the interlaminar capability of these type of joints. In this study, T-joints were manufactured using through-thickness stitching in dry carbon preforms and cured using the vacuum-assisted resin transfer molding (VARTM) process. Stitched and unstitched T-joints were tested under pull-off loading conditions, and surface strain fields were obtained using a 3D digital image correlation system. The ultimate load, displacement, and absorbed energy of the stitched T-joints were greater than their unstitched counterparts by approximately 16%, 34%, and 58%, respectively. Failure mechanisms were identified by examining fracture surfaces using optical microscopy. Results demonstrate that through-thickness stitching significantly improves the damage tolerance of T-joints, which highlights the effectiveness of stitching to enhance the structural integrity of large aerospace components.
VARTM↗
Development of a Fully Automated Guided Wave System for In-Process Cure Monitoring of CFRP Composite Laminates
A guided wave-based in-process cure monitoring technique for carbon fiber reinforced polymer (CFRP) composites was investigated at NASA Langley Research Center. A key cure transition point (vitrification) was identified and the degree of cure was monitored using metrics such as amplitude and time of arrival (TOA) of guided waves. Using an automated system preliminarily developed in this work, high-temperature piezoelectric transducers were utilized to interrogate a twenty-four ply unidirectional composite panel fabricated from Hexcel (Registered Trademark) IM7/8552 prepreg during cure. It was shown that the amplitude of the guided wave increased sharply around vitrification and the TOA curve possessed an inverse relationship with degree of cure. The work is a first step in demonstrating the feasibility of transitioning the technique to perform in-process cure monitoring in an autoclave, defect detection during cure, and ultimately a closed-loop process control to maximize composite part quality and consistency.
Hudson, Tyler B.↗
A study of the possible effect of a thermal post cure on the mechanical properties of the 404 carbon-phenolic ring of the space shuttle solid rocket motor nozzle
Erratic pockets of erosion have occurred on the inner perimeter of the 404 rocket nozzle ring during liftoff firing. It is thought that it may be caused by pockets of volatile matter entrapped during manufacture. A thermal post cure was suggested as a possible means of outgassing such pockets, if they in fact do exist. To confirm an outgassing during a post cure and to establish a working upper temperature limit, thermal gravimetric and differential calorimetric analyses were made on a number of samples from two 404 rings supplied by the manufacturer. Continuous weight loss was observed over the temperature range explored (750 F) indicating outgassing, and a strong exothermic reaction occurs beginning about 390 F. Thus, an upper post cure temperature of 350 F is recommended. To determine the possible effect of a post cure on physical properties, the following tests will be made on matched sets of cured and post cured material: x-radiography (internal structure), linear dimensions, weight, porosity, cross ply thermal expansion, drop and double notch shear strengths, and tensional strength in the ply direction.
Giardini, A. A.↗
Effects of cleavable comonomer structure and crosslinker chemistry on the performance and deconstructability of frontally cured pDCPD composites
Reclaiming undamaged carbon fiber from thermoset composites requires chemical recycling methods that leverage complete deconstruction of the polymer matrix. Cleavable comonomers enable chemical recycling of poly(dicyclopentadiene) (pDCPD) composites, but current systems suffer from reduced glass transition temperature (T g ), limiting application. Here, we investigate the effect of cleavable comonomer loading and cleavable crosslinker chemistry on network formation, thermomechanical properties, and fiber recovery in frontally cured pDCPD composites. All formulations fully deconstructed in acid and recovered fibers ranged from pristine to variably contaminated depending on crosslinker chemistry. Reducing backbone-cleaving comonomer content and introducing cleavable crosslinkers raised composite T g to 126–138 °C compared to 105 °C previously reported in deconstructable pDCPD composites. Although the cleavable crosslinkers increased T g in unreinforced polymers to 150–160 °C, the fiber-reinforced composite T g remained lower due to under-curing and interactions between the crosslinkers and the fiber surface. Increasing polymerization initiator loading improved comonomer conversion and yielded a deconstructable composite with T g = 151 °C, approaching the performance of non-deconstructable pDCPD composites (T g = 161 °C). This work clarifies how cleavable comonomer and crosslinker chemistry governs curing, thermomechanical performance, and reclaimed reinforcement quality, and the results highlight the need for more robust cleavable comonomers to realize multigenerational composite materials without sacrificing thermomechanical performance.
Carbon fibers↗
Cryogenic Durability of a Carbon Fiber Reinforced Cyanate Ester Composite: Degree-of-Cure Effect
The James Webb Space Telescope (JWST) will be located approximately 1.5 million kilometers from Earth, producing extremely cold temperatures on the optical portion of the observatory. Specifically, the Optical Telescope Element (OTE) and Integrated Science Instrument Module (ISIM) will operate at approximately -240 C. Construction of the structural components of the OTE and ISIM require bonding dissimilar materials together, e.g. Invar-36 (an iron-nickel alloy) to a carbon fiber reinforced cyanate ester composite (CFRCE) with an epoxy adhesive. While these materials enable the cryogenic stability required for optical performance, their joint strength at these extreme conditions presents a unique design challenge. Therefore, the current study presents a detailed investigation into the optimization of cryogenic composite durability. It is demonstrated that by controlling the degree-of-cure of a laminate, one can achieve an enhanced resistance to microcracking and an improved residual strength following cryogenic cycling to -253 C.
Polis, Daniel L.↗
Chemically and Mechanically Recyclable Vitrimers from Carbon Dioxide-Based Polycarbonates
Designing thermoset materials with dynamic crosslinks is an important strategy to mitigate rising global carbon dioxide emission levels. The development of polymers from sustainable feedstocks, with efficient manufacturing methods, for high-value applications, and with circular end-of-use solutions is essential for advancing material technologies. One approach involves exploiting carbon dioxide itself as feedstock to create high performance, sustainable materials, by enchaining 50 mol% CO2 via copolymerization with epoxides to yield polycarbonates. This work describes the synthesis, end-functionalization, and curing of poly(propylene carbonate) (PPC) and poly(cyclohexene carbonate) (PCHC) into beta-hydroxy ester vitrimers. These vitrimers demonstrate the ability to be mechanically reprocessed up to 3 times with retention of the material’s properties through dynamic transesterification exchange reactions. The polycarbonate vitrimers with gel fractions exceeding 90 % exhibit high tensile strength (> 50 MPa) and Young’s modulus (> 2 GPa), achieved by varying repeat unit structure in the polymer backbone from the low Tg PPC to the more rigid high Tg PCHC structures. Owing to an entropically favorable chain back-biting mechanism, the network chains can be cleaved and depolymerized into cyclic small molecules. In the case of PCHC, this process enables repolymerization back to polycarbonates with 69 wt.% CO2 retention through life-cycles. The promising mechanical performance and recyclability of these CO2-based polycarbonate vitrimers indicate their potential for sustainable, high-performance materials, paving the way for future innovations in circular polymer technologies and carbon capture utilization.
36 MATERIALS SCIENCE↗
A parametric study of accelerated carbonation in alkali-activated slag
Resistance to carbonation is one important attribute that low-CO{sub 2} cement alternatives must possess, and is particularly crucial for cement alternatives subjected to aggressive CO{sub 2} concentrations such as those used in construction of oil wells and wells for below ground carbon sequestration. Here, a parametric study of alkali-activated slag (AAS) carbonation in aggressive environments has been conducted to examine (i) calcium carbonate polymorphism using X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) spectroscopy, and (ii) the extent of calcium carbonate formation and CO{sub 2} adsorption using thermogravimetric analysis (TGA). A range of AASs have been studied by varying the magnesium content of the slag, the activator type (sodium hydroxide and sodium silicate), the activator concentration, and the curing time prior to carbonation. It was uncovered that both (i) magnesium from the slag and (ii) silica from the activating solution are needed to reduce the propensity for the sodium-containing calcium-alumino-silicate-hydrate gel to undergo decalcification.
36 MATERIALS SCIENCE↗
Additive manufacturing of carbon fiber-reinforced thermoset composites via in-situ thermal curing
Fiber-reinforced polymer composites are lightweight structural materials widely used in the transportation and energy industries. Current approaches for the manufacture of composites require expensive tooling and long, energy-intensive processing, resulting in a high cost of manufacturing, limited design complexity, and low fabrication rates. Here, we report rapid, scalable, and energy-efficient additive manufacturing of fiber-reinforced thermoset composites, while eliminating the need for tooling or molds. Use of a thermoresponsive thermoset resin as the matrix of composites and localized, remote heating of carbon fiber reinforcements via photothermal conversion enables rapid, in-situ curing of composites without further post-processing. Rapid curing and phase transformation of the matrix thermoset, from a liquid or viscous resin to a rigid polymer, immediately upon deposition by a robotic platform, allows for the high-fidelity, freeform manufacturing of discontinuous and continuous fiber-reinforced composites without using sacrificial support materials. This method is applicable to a variety of industries and will enable rapid and scalable manufacture of composite parts and tooling as well as on-demand repair of composite structures.
36 MATERIALS SCIENCE↗
Carbon composition with hierarchical porosity, and methods of preparation
A method for fabricating a porous carbon material possessing a hierarchical porosity, the method comprising subjecting a precursor composition to a curing step followed by a carbonization step, the precursor composition comprising: (i) a templating component comprised of a block copolymer, (ii) a phenolic component, (iii) a dione component in which carbonyl groups are adjacent, and (iv) an acidic component, wherein said carbonization step comprises heating the precursor composition at a carbonizing temperature for sufficient time to convert the precursor composition to a carbon material possessing a hierarchical porosity comprised of mesopores and macropores. Also described are the resulting hierarchical porous carbon material, a capacitive deionization device in which the porous carbon material is incorporated, as well as methods for desalinating water by use of said capacitive deionization device.
36 MATERIALS SCIENCE↗
Predicting Saturated Hydraulic Conductivity over Time for Degrading Saltstone Vault Concrete - 20376
At the Savannah River Site (SRS), low-level liquid tank waste is mixed with cementitious materials to produce a solid, monolithic waste form referred to as saltstone. The liquid saltstone mixture is pumped into massive concrete structures referred to as saltstone disposal units (SDUs) for curing and long-term storage. SDUs are vaults made of high performance concrete forming a barrier between saltstone and the surrounding environment. Predicting the long-term performance of SDU vault concrete, as well as the saltstone material itself, is critical to understanding the potential releases of radionuclides to the surrounding environment as described in the Saltstone Disposal Facility (SDF) performance assessment (PA). The hydraulic conductivity profile for SDU vault concrete was conservatively assumed to degrade linearly from the initial saturated hydraulic conductivity of the intact concrete over a long period of time. The initial hydraulic properties of saturated SDU vault concrete have been measured, and the final hydraulic properties of degraded vault concrete are assumed to be the same as the porous backfill material that will surround the vault after closure. The assumed final condition of the vault concrete is also conservative in that it provides a greater estimate of water penetration through the vault than would generally be expected. Therefore, insights that provide more realistic but conservative estimates as to how degradation processes may change the hydraulic properties of the SDU vault concrete, the time dependent relationship of the vault concrete hydraulic properties to degradation (and thus time), and the final hydraulic properties of the vault concrete provides useful additions to the SDF PA. This paper focuses on the assumption that the saltstone vault concrete saturated hydraulic conductivity would decrease linearly as a function of degradation time; this assumption resulted from a worst-case, weighted (by relative layer thickness), arithmetic average of intact and backfill material hydraulic conductivities representing flow parallel to a layered system. This research indicates that the effective saturated hydraulic conductivity of the degraded SDU vault concrete should be based on the relative thickness-weighted geometric mean of the intact and degraded layers hydraulic conductivities. This alternative, which is supported extensively in the relevant literature and evaluated in this paper, leads to a more realistic and defensible estimate of the effective saturated hydraulic conductivity in degraded vault concrete while remaining conservative. The impact of using the more realistic estimate of the effective saturated hydraulic conductivity for the degraded concrete decreases the effective saturated hydraulic conductivity by up to several orders of magnitude for early times (i.e., when the SDU vault concrete is assumed degraded via sulfate attack and carbonation). This revised estimate of the effective saturated hydraulic conductivity has been implemented in the recently revised SDF PA. (authors)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Through Thickness Thermal Gradients in Thick Laminates During Cure, Influence on Tg and Modulus
Carbon fiber composites are materials of great interest to the aerospace industry because of their light weight and high strength properties. Composite use in high load bearing applications such as roto-craft gearing requires manufacturing parts that are 1.5 inches thick and beyond. Very thick composite parts (laminates) produce thermal gradients and temperature spikes due to the heat released by resin polymerization and cross-linking during composite cure. It is believed that these thermal gradients will cause internal stresses to build-up inside these ultra-thick laminates during the cure-cycle, yielding parts with non-uniform mechanical properties throughout the thickness of the laminate. The goal of this study is to identify these thermal gradients and determine the magnitude of difference in mechanical properties generated by them.
Mechanical Properties↗
Carbon microsphere-filled Pyrrone foams.
Syntactic foam formulations were prepared from mixtures of Pyrrone prepolymers and hollow carbon microspheres. Very low curing shrinkages were obtained for high volume loadings of microspheres. The resulting syntactic foams were found to be remarkably stable over a wide range in temperature. A technique was developed for the emplacement of these foam formulations in polyimide-fiberglass, titanium alloy and stainless steel honeycomb without sacrificing low curing shrinkage or thermal stability.
Kimmel, B. G.↗
High performance, rapid thermal/UV curing epoxy resin for additive manufacturing of short and continuous carbon fiber epoxy composites
An additive manufacturing resin system includes a container; a build platform in the container; a build platform drive; an additive manufacturing resin that forms an additive manufacturing resin bath; an additive manufacturing print head; a build material supply connected to the additive manufacturing print head; an infill resin in the container, wherein the infill resin is supported by the additive manufacturing resin bath; a computer controller; and an extruded material that forms the product, wherein the infill resin at least partially surrounds the extruded material that forms the product. An infill resin supply provides the infill resin into the container and a control valve is connected to the infill resin supply. An IR light sensor is connected to the control valve and operatively connected to the infill resin in the container.
Lewicki, James↗
No-Oven, No-Autoclave Composite Processing
Very large composite structures, such as those used in NASA's Space Launch System, push the boundaries imposed by current autoclaves. New technology is needed to maintain composite performance and free manufacturing engineers from the restraints of curing equipment size limitations. Recent efforts on a Phase II project by Cornerstone Research Group, Inc. (CRG), have advanced the technology and manufacturing readiness levels of a unique two-part epoxy resin system. Designed for room-temperature infusion of a dry carbon preform, the system includes a no-heat-added cure that delivers 350 F composite performance in a matter of hours. This no-oven, no-autoclave (NONA) composite processing eliminates part-size constraints imposed by infrastructure and lowers costs by increasing throughput and reducing capital-specific, process-flow bottlenecks. As a result of the Phase II activity, NONA materials and processes were used to make high-temperature composite tooling suitable for further production of carbon-epoxy laminates and honeycomb/ sandwich-structure composites with an aluminum core. The technology platform involves tooling design, resin infusion processing, composite part design, and resin chemistry. The various technology elements are combined to achieve a fully cured part. The individual elements are not unusual, but they are combined in such a way that enables proper management of the heat generated by the epoxy resin during cure. The result is a self-cured carbon/ epoxy composite part that is mechanically and chemically stable at temperatures up to 350 F. As a result of the successful SBIR effort, CRG has launched NONA Composites as a spinoff subsidiary. The company sells resin to end users, fabricates finished goods for customers, and sells composite tooling made with NONA materials and processes to composite manufacturers.
Rauscher, Michael D.↗
Design of highly damage-tolerant sandwich panels
The effects of different fabrication procedures to increase the damage tolerance of sandwich panels were studied. Baseline panels consisted of a 25.4 mm premolded core, surfaced with 177 C cure film adhesive and carbon-bismaleimide prepreg which were subsequently cocured onto the core. It was found that panels with a prefabricated skin, which was subsequently bonded onto the core with room temperature cure adhesive, showed greatly increased damage tolerance.
Hiel, Clement↗